CN111499414B - Light high-strength scouring-resistant ceramic heat-insulation integrated structure and preparation method thereof - Google Patents
Light high-strength scouring-resistant ceramic heat-insulation integrated structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a light high-strength scouring-resistant ceramic heat-insulation integrated structure and a preparation method thereof, wherein the heat-insulation integrated structure comprises the following components: a reinforced light anti-oxidation porous heat insulation matrix structure and a compact scour-resistant heat-proof coating coated on the surface of the porous matrix; the matrix structure is a low-heat-conduction porous anti-oxidation ceramic fiber heat insulation structure which is subjected to siloxane colloid impregnation and pyrolysis treatment, and the main components of the matrix structure are aluminum oxide and silicon oxide; the coating is a refractory metal silicide coating system with oxidation resistance, and the main components of the coating are molybdenum disilicide, tantalum disilicide, silicon oxide and boron oxide; and coating a compact scouring-resistant coating on the surface of the reinforced light porous antioxidant heat-insulating matrix structure and sintering to obtain the integrated light heat-insulating structure. The invention overcomes the problems of large brittleness, poor impact resistance, low temperature resistance, incompatible interfaces between the heat-proof double-layer structures and the like of the ceramic heat-insulating structure, and has the characteristics of high temperature resistance, low density, high strength, strong scouring resistance, good stability, simple preparation process and the like.
Description
Technical Field
The invention relates to a light high-strength scouring-resistant ceramic heat-insulation integrated structure and a preparation method thereof, belonging to the technical field of ceramic heat-insulation structures.
Background
The new generation of aircraft becomes an important strategic weapon equipment for competitive development of military and strong countries in the 21 st century by the characteristics of hypersonic cruise, quick maneuvering reaction, high reliability, low maintenance cost and the like. Aircraft with the background of X-37B and space shuttle are exposed to a very harsh thermal environment during long-term flight and reentry in the near space, and the surface temperature of the local parts (such as the head and the leading edge) of the aircraft is very high, thus posing a serious challenge to the thermal protection structure and materials of the aircraft. Carbon/carbon composites, ceramic heat protection tiles, ceramic heat insulation tiles, ultra high temperature ceramics are the most prominent heat protection candidate materials in such aircraft thermal protection systems. However, the carbon/carbon composite material has the problem of easy ablation at high temperature, the ultrahigh-temperature ceramic also has the problem of easy cracking, the ceramic heat-proof tile and the ceramic heat-insulating tile also have the problems of low temperature resistance, large brittleness, poor scouring resistance and the like, and the ceramic heat-proof tile and the ceramic heat-insulating tile also have the problem of compatibility.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcome prior art's not enough, provide a light high strength resistant ceramic of erodeing and prevent thermal-insulated integrated structure, solved the problem that traditional pottery heat protection tile, pottery heat insulation tile exist.
The technical solution of the invention is as follows:
the utility model provides a thermal-insulated integral structure is prevented to resistant ceramic of erodeing of light high strength, includes: the heat insulation structure comprises a matrix structure (1) and a coating (2) coated on the surface of the matrix structure, wherein the matrix structure (1) is a reinforced porous anti-oxidation ceramic fiber heat insulation structure, and the coating (2) is a refractory metal silicide coating with oxidation resistance.
Furthermore, the reinforced porous antioxidant ceramic fiber is porous antioxidant ceramic fiber subjected to siloxane colloid impregnation pyrolysis treatment, and the structural equivalent density is lower than 400kg/cm3The thermal conductivity is lower than 0.2W/m.K.
Further, the reinforced porous oxidation-resistant ceramic fiber comprises the components of aluminum oxide and silicon oxide; the total content of the aluminum oxide and the silicon oxide in percentage by weight is more than 95 percent, wherein the content of the aluminum oxide in percentage by weight is 50-80 percent.
Further, the preparation process of the reinforced porous antioxidant ceramic fiber comprises the following steps: the porous oxidation-resistant matrix structure is soaked in siloxane colloid for 10 minutes to 6 hours, then is placed in the air for 6 to 48 hours, and is sintered in an aerobic atmosphere for 12 to 24 hours.
Further, the coating (2) comprises silicon oxide, boron oxide, molybdenum disilicide and tantalum disilicide, and the mass ratio of the coating components is 1: 1-4: 1-10: 1 to 5.
Further, after the surface of the strengthened matrix structure is coated with the coating (2), the matrix structure is placed in the air for 12-48 hours and then sintered in an aerobic atmosphere, wherein the sintering highest temperature is 1000-1500 ℃, and the anti-heat-insulation integrated structure is obtained.
Further, the coating (2) is partially immersed into the reinforced porous oxidation-resistant ceramic fiber to form a gradient structure.
Furthermore, the thickness of the coating (2) is 100 um-2 mm, and the thickness of the matrix structure is not less than 5 mm.
Further, the equivalent density of the heat-proof and heat-insulation integrated structure is lower than 500kg/cm3The compression strength is not lower than 1.5MPa, and the temperature resistance is more than 1700 ℃.
Furthermore, the invention also provides a preparation method of the heat-proof and heat-insulation integrated structure, which comprises the following steps:
(1) preparing a matrix structure; the matrix structure is a porous anti-oxidation ceramic fiber structure and is prepared by alumina and silica; the total content of the alumina and the silicon oxide in percentage by weight is more than 95 percent, wherein the content of the alumina in percentage by weight is 50-80 percent;
(2) strengthening and sintering the base structure; soaking the porous oxidation-resistant matrix structure in siloxane colloid for 10 minutes to 6 hours, then placing the porous oxidation-resistant matrix structure in the air for 6 to 48 hours, and sintering the porous oxidation-resistant matrix structure in an aerobic atmosphere for 12 to 24 hours; the thickness of the matrix structure is not less than 5 mm;
(3) preparing coating slurry: preparing coating slurry by using silicon oxide, boron oxide, molybdenum disilicide and tantalum disilicide, wherein the coating slurry comprises the following components in percentage by mass: 1-4: 1-10: 1-5;
(4) coating the coating slurry on the reinforced sintered base structure so that part of the coating slurry is impregnated into the reinforced sintered base structure; the thickness of the coating is 100 um-2 mm;
(5) and (3) placing the material in the air for 12-48 hours, and then sintering the material in an aerobic atmosphere, wherein the sintering highest temperature is 1000-1500 ℃, so as to obtain the heat-proof and heat-insulating integrated structure.
Compared with the prior art, the invention has the beneficial effects that:
(1) the integrated design of heat insulation and prevention of the invention is different from the prior ablation carbon-carbon composite material system and the heat insulation and prevention double-layer structure, and the substrate material of the invention selects the ceramic material system with the anti-oxidation function, thereby avoiding the anti-oxidation problem. And the heat-proof and heat-insulating integrated design is selected, so that the compatibility problem caused by the traditional heat-proof and heat-insulating double-layer design is avoided.
(2) The invention improves the brittleness of the matrix ceramic heat insulation material, realizes the heat insulation prevention integrated design of the whole structure, enhances the compression strength by several times, increases the temperature resistance under high-strength scouring from hundreds of KPa magnitude orders to MPa, and exceeds 1700 ℃ of the temperature resistance under high-strength scouring, improves the temperature resistance and the scouring resistance, and ensures that the matrix heat insulation structure has the heat prevention function. The density of the whole structure is lower than 500g/cm3, and the density is about 1/3 of the existing carbon-carbon composite material.
(3) According to the invention, the compact high-temperature-resistant oxidation-resistant coating is coated on the surface of the reinforced porous heat-insulating matrix structure, so that the scouring resistance and the temperature resistance of the whole structure are improved. Thereby solving the problems of large brittleness, non-compact surface, low temperature resistance, incompatible interface between the heat-proof and heat-insulating double-layer structures and the like of the light porous ceramic heat-insulating structure; the prepared integrated heat-proof and heat-insulating structure has the characteristics of high temperature resistance, low density, high strength, strong scouring resistance, good stability, simple preparation process and the like.
Drawings
FIG. 1 is a schematic view of an integrated structure of the present invention for preventing and insulating heat;
FIG. 2 is a diagram of an integrated structure of the present invention;
FIG. 3 is a diagram of the heat-proof integrated structure of the invention after examination;
FIG. 4 is a surface temperature response diagram of the integrated structure for preventing and insulating heat;
FIG. 5 is a strength diagram of the integrated structure of the present invention.
Detailed Description
The following further describes the embodiments of the present invention with reference to the drawings.
The invention designs and prepares a light high-strength scouring-resistant ceramic heat-insulation integrated structure: the compatibility problem between the heat-proof layer and the heat-insulating layer is avoided through the heat-proof and heat-insulating integrated design; the light anti-oxidation heat insulation base material is selected, so that the anti-oxidation problem of the traditional heat insulation material is avoided, and the light requirement in the heat insulation design is met; the strength of the porous heat insulation matrix structure is improved by strengthening the light porous matrix material; the compact high-temperature-resistant oxidation-resistant coating is coated on the surface of the reinforced porous heat-insulating matrix structure, so that the scouring resistance and the temperature resistance of the whole structure are improved. Thereby solving the problems of large brittleness, non-compact surface, low temperature resistance, incompatible interface between the heat-proof and heat-insulating double-layer structures and the like of the light porous ceramic heat-insulating structure; the prepared integrated heat-proof and heat-insulating structure has the characteristics of high temperature resistance, low density, high strength, strong scouring resistance, good stability, simple preparation process and the like.
As shown in fig. 1, the present invention provides a high-strength erosion-resistant lightweight ceramic heat-proof integrated structure, comprising: a reinforced light anti-oxidation ceramic fiber heat insulation matrix structure 1 and a compact high temperature resistant high heat conduction coating 2 coated on the surface of the matrix structure. Preferably, the equivalent density of the heat-insulation integrated structure is lower than 500kg/cm3, the compression strength is not lower than 1.5MPa, and the temperature resistance is higher than 1700 ℃.
Preferably, the thickness of the coating is 100 um-2 mm, the inside is a reinforced porous fiber heat insulation structure, and the thickness of the matrix structure is not less than 5 mm.
Preferably, the reinforced porous antioxidant ceramic fiber is prepared by impregnating and pyrolyzing the porous antioxidant ceramic fiber with siloxane colloid, has a structural equivalent density of less than 400kg/cm3, and has a thermal conductivity of less than 0.2W/m.K. The main components of the aluminum oxide-silicon composite material are aluminum oxide and silicon oxide, and the total content of the aluminum oxide and the silicon oxide is more than 95 percent (mass percent), wherein the content of the aluminum oxide is 50 to 80 percent (mass percent).
The preparation process of the reinforced porous antioxidant ceramic fiber comprises the following steps: the porous oxidation-resistant matrix structure is soaked in siloxane colloid for 10 minutes to 6 hours, then is placed in the air for 6 to 48 hours, and is sintered in an aerobic atmosphere for 12 to 24 hours.
Preferably, the coating material on the surface of the substrate is a refractory metal silicide coating system with oxidation resistance, the main components are silicon oxide, boron oxide, molybdenum disilicide and tantalum disilicide, and the mass ratio of the coating components is 1: 1-4: 1-10: 1 to 5. Molybdenum disilicide and tantalum disilicide used on the surface of the substrate are both high-temperature-resistant and oxidation-resistant materials and can be used as substrate materials of the coating; the silicon oxide and boron oxide are helpful for forming a glass phase so as to form a compact glass surface, and simultaneously, the temperature gradient of the coating and the matrix structure can be relieved. The internal components of the coating are partially impregnated into the porous matrix to form a graded structure to mitigate thermal expansion coefficient mismatch between the coating and the matrix.
Coating refractory metal silicide coating slurry on the surface of the reinforced matrix structure, placing the matrix structure in air for 12-48 hours, and finally sintering the matrix structure in an aerobic atmosphere, wherein the highest sintering temperature is 1000-1500 ℃.
The invention also provides a method for preparing the heat-proof and heat-insulation integrated structure, which comprises the following steps:
(1) preparing a matrix structure; the matrix structure is a porous anti-oxidation ceramic fiber structure and is prepared by alumina and silica; the total content of the alumina and the silicon oxide in percentage by weight is more than 95 percent, wherein the content of the alumina in percentage by weight is 50-80 percent;
(2) strengthening and sintering the base structure; soaking the porous oxidation-resistant matrix structure in siloxane colloid for 10 minutes to 6 hours, then placing the porous oxidation-resistant matrix structure in the air for 6 to 48 hours, and sintering the porous oxidation-resistant matrix structure in an aerobic atmosphere for 12 to 24 hours; the thickness of the matrix structure is not less than 5 mm;
(3) preparing coating slurry: preparing coating slurry by using silicon oxide, boron oxide, molybdenum disilicide and tantalum disilicide, wherein the coating slurry comprises the following components in percentage by mass: 1-4: 1-10: 1-5;
(4) coating the coating slurry on the reinforced sintering matrix structure, so that part of the coating slurry is impregnated into the reinforced sintering matrix structure; the thickness of the coating is 100 um-2 mm;
(5) and (3) placing the material in the air for 12-48 hours, and then sintering the material in an aerobic atmosphere, wherein the sintering highest temperature is 1000-1500 ℃, so as to obtain the heat-proof and heat-insulating integrated structure.
The heat-insulating layer is integrally designed, so that the problem of compatibility between the heat-insulating layer and the heat-insulating layer is solved. Improves the brittleness of ceramic heat-insulating materials, realizes the integrated functions of heat prevention and heat insulation, and improves the temperature resistance and the scouring resistance
The following examples of the present invention are given:
FIG. 1 is a schematic structural view of an embodiment of an integrated heat insulation structure of the present invention.
The matrix structure 1 is a porous oxidation-resistant ceramic fiber, the main components of which are alumina and silica, and the content of the alumina and the silica is 99 percent (mass percent), wherein the content of the alumina is 80 percent (mass percent). The coating structure 2 is a ceramic coating, the main components are silicon dioxide, boron oxide, molybdenum disilicide and tantalum disilicide, and the mass ratio of the coating components is 1: 1: 5: 1.
the base structure was immersed in the silicone gel for 3 hours, then left to stand in air for 48 hours, and sintered in an aerobic atmosphere for 24 hours.
Coating refractory metal silicide coating slurry on the surface of the strengthened matrix structure, standing in the air for 36 hours, and finally sintering in an aerobic atmosphere at the highest sintering temperature of 1200 ℃ to obtain the lightweight high-strength scouring-resistant ceramic heat-insulation integrated structure.
Fig. 2 shows a physical diagram of a high-strength erosion-resistant ceramic heat-proof integrated structure designed according to fig. 1. The surface is compact and uniform.
In order to better explain the temperature resistance and the scouring resistance of the high-strength scouring-resistant ceramic heat-insulation integrated structure, the temperature resistance of the physical diagram in FIG. 2 is examined, and the examined model surface is complete, as shown in FIG. 3.
Fig. 4 shows the model surface temperature response after examination, the model surface temperature exceeding 1700 ℃.
In order to better illustrate the strength improvement effect of the designed high-strength scouring-resistant ceramic heat-insulation integrated structure, a strength test was performed on a standard block structure of 20mm by 20mm, and fig. 5 shows the strength comparison of the prepared high-strength scouring-resistant ceramic heat-insulation integrated structure: the compressive strength of the reinforced heat-insulation integrated structure is obviously improved compared with that of the matrix structure, and the strength reaches the MPa magnitude.
In summary, the light high-strength scouring-resistant ceramic heat-insulation integrated structure is different from the existing ablation carbon-carbon composite material system, and the substrate material of the light high-strength scouring-resistant ceramic heat-insulation integrated structure selects a ceramic material system with an anti-oxidation function, so that the anti-oxidation problem is avoided. And the heat-proof and heat-insulating integrated design is selected, so that the compatibility problem caused by the traditional heat-proof and heat-insulating double-layer design is avoided. The brittleness of the matrix ceramic heat insulation material is improved, the heat insulation integrated design of the whole structure is realized, the compression strength is enhanced by several times, the temperature resistance under high-strength scouring is more than 1700 ℃ from hundreds of KPa magnitude orders to MPa, the temperature resistance and scouring resistance are improved, and the matrix heat insulation material has the heat insulation function. The density of the whole structure is lower than 500g/cm3The density of the carbon-carbon composite material is about 1/3 of the existing carbon-carbon composite material, the process is simple and feasible, the development period is short, and the development cost is low.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (4)
1. The utility model provides a thermal-insulated integral structure is prevented to resistant pottery that erodees of light high strength which characterized in that includes: the heat insulation structure comprises a matrix structure (1) and a coating (2) coated on the surface of the matrix structure, wherein the matrix structure (1) is a reinforced porous anti-oxidation ceramic fiber heat insulation structure, and the coating (2) is a refractory metal silicide coating with oxidation resistance;
the reinforced porous oxidation-resistant ceramic fiber comprises the components of aluminum oxide and silicon oxide; the total content of the alumina and the silicon oxide in percentage by weight is more than 95 percent, wherein the content of the alumina in percentage by weight is 50-80 percent;
the coating (2) comprises silicon oxide, boron oxide, molybdenum disilicide and tantalum disilicide, and the mass ratio of the coating components is 1: 1-4: 1-10: 1-5;
after the surface of the reinforced matrix structure is coated with the coating (2), the matrix structure is placed in the air for 12 to 48 hours and then sintered in an aerobic atmosphere, wherein the sintering highest temperature is 1000 to 1500 ℃, and the anti-heat-insulation integrated structure is obtained;
the coating (2) is partially immersed into the reinforced porous oxidation-resistant ceramic fiber to form a gradient structure;
the thickness of the coating (2) is 100 um-2 mm, and the thickness of the matrix structure is not less than 5 mm;
the equivalent density of the heat-proof and heat-insulation integrated structure is lower than 500kg/cm3The compression strength is not lower than 1.5MPa, and the temperature resistance is more than 1700 ℃.
2. The light high-strength scouring-resistant ceramic heat-proof and heat-insulation integrated structure as claimed in claim 1, wherein: the reinforced porous antioxidant ceramic fiber is a porous antioxidant ceramic fiber subjected to siloxane colloid impregnation pyrolysis treatment, and the equivalent density of the porous antioxidant ceramic fiber is lower than 400kg/cm3The thermal conductivity is lower than 0.2W/m.K.
3. The light high-strength scouring-resistant ceramic heat-proof and heat-insulation integrated structure as claimed in claim 1, wherein: the preparation process of the reinforced porous antioxidant ceramic fiber comprises the following steps: the porous oxidation-resistant matrix structure is soaked in siloxane colloid for 10 minutes to 6 hours, then is placed in the air for 6 to 48 hours, and is sintered in an aerobic atmosphere for 12 to 24 hours.
4. A method for preparing a lightweight high-strength erosion-resistant ceramic heat-proof and heat-insulation integrated structure as claimed in any one of claims 1 to 3, characterized by comprising the following steps:
(1) preparing a matrix structure; the matrix structure is a porous anti-oxidation ceramic fiber structure and is prepared by alumina and silica; the total content of the alumina and the silicon oxide in percentage by weight is more than 95 percent, wherein the content of the alumina in percentage by weight is 50-80 percent;
(2) strengthening and sintering the base structure; soaking the porous oxidation-resistant matrix structure in siloxane colloid for 10 minutes to 6 hours, then placing the porous oxidation-resistant matrix structure in the air for 6 to 48 hours, and sintering the porous oxidation-resistant matrix structure in an aerobic atmosphere for 12 to 24 hours; the thickness of the matrix structure is not less than 5 mm;
(3) preparing coating slurry: preparing coating slurry by using silicon oxide, boron oxide, molybdenum disilicide and tantalum disilicide, wherein the mass ratio of the components is 1: 1-4: 1-10: 1-5;
(4) coating the coating slurry on the reinforced sintered base structure so that part of the coating slurry is impregnated into the reinforced sintered base structure; the thickness of the coating is 100 um-2 mm;
(5) and (3) placing the material in the air for 12-48 hours, and then sintering the material in an aerobic atmosphere, wherein the sintering highest temperature is 1000-1500 ℃, so as to obtain the heat-proof and heat-insulating integrated structure.
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| CN101863683A (en) * | 2009-04-15 | 2010-10-20 | 中国科学院上海硅酸盐研究所 | Anti-oxidation coating and preparation method thereof |
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